CN105525292A - Nanometer-titania-based preparing method for etching liquid for circuit board - Google Patents
Nanometer-titania-based preparing method for etching liquid for circuit board Download PDFInfo
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- CN105525292A CN105525292A CN201510946534.8A CN201510946534A CN105525292A CN 105525292 A CN105525292 A CN 105525292A CN 201510946534 A CN201510946534 A CN 201510946534A CN 105525292 A CN105525292 A CN 105525292A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
Abstract
The invention discloses a nanometer-titania-based preparing method for etching liquid for a circuit board. The etching liquid includes, by weight percentage, 3.5%-6.5% of nanometer titania, 0.5%-1.2% of ferric trichloride, 0.5%-1.6% of nitric acid, 2.5%-3.3% of organic hydrochloric acid, 1.5%-2.3% of a non-ionic surface active agent, 0.5%-1.5% of a stabilizer, 3.5%-5.6% of a defoamer and the balance distilled water. According to the method, the nanometer titania is newly added on the basis of an original process, etching can be carried out under the condition that etch-resistant coating permeation does not occur, the etching speed of a chromium metal film is obviously increased, the controllability of the etching speed is achieved, degradation of the anti-corrosion protective layer is effectively restrained, chromium metal film wires with smooth surfaces are obtained, and the important application value is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of the circuit card etching solution based on nano titanium oxide.
Background technology
At present in the process of circuit board manufacturing, the quality of quality of circuit board, the discovery of quality problem and solution, the assessment that processing procedure improves all needs to be come its objective determination and judgement by microsection.The quality that microsection makes directly has influence on the quality evaluation of circuit card.Traditional microsection process comprises, and samples by the mode of milling; Resin inlaying process is adopted to carry out sealing to sample; Sample is ground; Polishing is carried out to sample; Microetch is carried out to sample.Wherein, the formula of micro etching solution is mass percent is 2 ~ 3, the hydrogen peroxide of 50%, the ammoniacal liquor 8ml of 25% ~ 28%, deionized water (Deionizedwater is called for short DI water) 8ml.Its shortcoming is, the volatile and irritant smell of the ammoniacal liquor in this micro etching solution, is therefore unfavorable for operation, and the time used after configuration is short, can only maintain 0.5 hours, thus brings inconvenience to the technique of microsection.
Summary of the invention
The defect that the present invention seeks to exist for prior art provides a kind of preparation method of the circuit card etching solution based on nano titanium oxide.
The present invention for achieving the above object, adopts following technical scheme: a kind of preparation method of the circuit card etching solution based on nano titanium oxide, comprises the steps:
The first step: weakly acidic cation-exchange resin being joined weight percent is in 2.5% ~ 3.3% organic hydrochloric acid, be uniformly mixed, the speed stirred is 50 ~ 60 revs/min, churning time is 5 ~ 7 minutes, whipping temp is 10 ~ 13 DEG C, then leach weakly acidic cation-exchange resin, control or remove the foreign ion in organic hydrochloric acid;
Second step: be that the nano titanium oxide of 2.5 ~ 4.5% and the distilled water of 1/3rd are to entering in reactor by weight percent, fully stir under normal temperature, normal pressure, churning time is 10 ~ 12 minutes, and stirring velocity is 60 ~ 70 revs/min, and whipping temp is 12 ~ 14 DEG C;
3rd step: then add the iron trichloride that weight percent is 0.5% ~ 1.2%, fully stir 6 ~ 7 minutes; Add the nitric acid that weight percent is 0.5 ~ 1.6%, fully stir 5 ~ 7 minutes; Add the distilled water of 1/3rd, fully stir 4 ~ 6 minutes; Add organic hydrochloric acid that weight percent is 2.5 ~ 3.3%, fully stir 5 ~ 7 minutes; Add the nonionogenic tenside that weight percent is 1.5 ~ 2.3%, fully stir 4 ~ 6 minutes; Add the stablizer that weight percent is 0.5 ~ 1.5%; Add the defoamer that weight percent is 3.5 ~ 5.6%, fully stir 3 ~ 7 minutes; Finally add residue distilled water again, then stir 8 ~ 10 minutes, stirring velocity is 45 ~ 55 revs/min, and whipping temp is 14 ~ 18 DEG C;
4th step: finally by the metre filter of obtained mixture through 0.12 μm, to remove the unwanted particles that particle diameter in mixture is greater than 0.12 μm, obtained required etching solution, its surface tension is low is 20 ~ 40 × 10-3N/m.
Further, the concentration of described nitric acid is greater than 97.5% (weight percent), and the concentration of described organic hydrochloric acid is greater than 89% (weight percent).
Further, described nonionogenic tenside is spans nonionogenic tenside.
Further, described weakly acidic cation-exchange resin is slightly acidic vinylbenzene Zeo-karb.
Further, the mass ratio of described weakly acidic cation-exchange resin and organic hydrochloric acid is 0.3 ~ 0.5.
Beneficial effect of the present invention: the present invention by newly adding nano titanium oxide on the basis of original technique, can not only etch when there is not etch-resistant coating infiltration, significantly improve the etching speed of chromium metallic membrane, there is etching speed controllability, the deterioration of effective suppression anticorrosion protection layer, obtain the chromium metallic membrane distribution of surperficial flat-satin, there is important using value; And effectively can reduce the surface tension of etching solution, infiltration can not only be produced, the effect infiltrated, and can etching indium tin oxide semiconductor nesa coating speed moderate, stable reaction, makes it under the prerequisite not affecting quality product, improve the etch effect of product, and product can be preserved at relatively low ambient temperatures, avoid the etching that original technology causes clean, the shortcoming that can not store at low temperatures, present method can be applicable to scale operation.
Embodiment
Embodiment 1
The preparation method of foregoing circuit plate etching solution, comprises the steps:
The first step: weakly acidic cation-exchange resin being joined weight percent is in 2.5% organic hydrochloric acid, be uniformly mixed, the speed stirred is 50 revs/min, churning time is 5 minutes, whipping temp is 10 DEG C, then leach weakly acidic cation-exchange resin, control or remove the foreign ion in organic hydrochloric acid;
Second step: by weight percent be the nano titanium oxide of 2.5% and the distilled water of 1/3rd to entering in reactor, fully stir under normal temperature, normal pressure, churning time is 10 minutes, and stirring velocity is 60 revs/min, and whipping temp is 12 DEG C;
3rd step: then add the iron trichloride that weight percent is 0.5%, fully stirs 6 minutes; Add the nitric acid that weight percent is 0.5%, fully stir 5 minutes; Add the distilled water of 1/3rd, fully stir 4 minutes; Add organic hydrochloric acid that weight percent is 2.5%, fully stir 5 minutes; Add the nonionogenic tenside that weight percent is 1.5%, fully stir 4 minutes; Add the stablizer that weight percent is 0.5%; Add the defoamer that weight percent is 3.5%, fully stir 3 minutes; Finally add residue distilled water again, then stir 8 minutes, stirring velocity is 45 revs/min, and whipping temp is 14 DEG C;
4th step: finally by the metre filter of obtained mixture through 0.12 μm, to remove the unwanted particles that particle diameter in mixture is greater than 0.12 μm, obtained required etching solution, its surface tension is low is 40 × 10
-3n/m.
Wherein, the concentration of described nitric acid is greater than 97.5% (weight percent), and the concentration of described organic hydrochloric acid is greater than 89% (weight percent).
Wherein, described nonionogenic tenside is spans nonionogenic tenside.
Wherein, described weakly acidic cation-exchange resin is slightly acidic styrene type cation exchange resin.
Wherein, the mass ratio of described weakly acidic cation-exchange resin and organic hydrochloric acid is 0.2 ~ 0.5.
Embodiment 2
The preparation method of foregoing circuit plate etching solution, comprises the steps:
The first step: weakly acidic cation-exchange resin being joined weight percent is in 2.8% organic hydrochloric acid, be uniformly mixed, the speed stirred is 55 revs/min, churning time is 6 minutes, whipping temp is 12 DEG C, then leach weakly acidic cation-exchange resin, control or remove the foreign ion in organic hydrochloric acid;
Second step: by weight percent be the nano titanium oxide of 3.5% and the distilled water of 1/3rd to entering in reactor, fully stir under normal temperature, normal pressure, churning time is 11 minutes, and stirring velocity is 65 revs/min, and whipping temp is 13 DEG C;
3rd step: then add the iron trichloride that weight percent is 0.8%, fully stirs 7 minutes; Add the nitric acid that weight percent is 1.0%, fully stir 6 minutes; Add the distilled water of 1/3rd, fully stir 5 minutes; Add organic hydrochloric acid that weight percent is 2.8%, fully stir 6 minutes; Add the nonionogenic tenside that weight percent is 1.9%, fully stir 5 minutes; Add the stablizer that weight percent is 0.9%; Add the defoamer that weight percent is 4.6%, fully stir 5 minutes; Finally add residue distilled water again, then stir 9 minutes, stirring velocity is 49 revs/min, and whipping temp is 15 DEG C;
4th step: finally by the metre filter of obtained mixture through 0.12 μm, to remove the unwanted particles that particle diameter in mixture is greater than 0.12 μm, obtained required etching solution, its surface tension is low is 30 × 10
-3n/m.
Wherein, the concentration of described nitric acid is greater than 97.5% (weight percent), and the concentration of described organic hydrochloric acid is greater than 89% (weight percent).
Wherein, described nonionogenic tenside is spans nonionogenic tenside.
Wherein, described weakly acidic cation-exchange resin is slightly acidic styrene type cation exchange resin.
Wherein, the mass ratio of described weakly acidic cation-exchange resin and organic hydrochloric acid is 0.2 ~ 0.5.
Embodiment 3
The preparation method of foregoing circuit plate etching solution, comprises the steps:
The first step: weakly acidic cation-exchange resin being joined weight percent is in 2.8% organic hydrochloric acid, be uniformly mixed, the speed stirred is 60 revs/min, churning time is 7 minutes, whipping temp is 13 DEG C, then leach weakly acidic cation-exchange resin, control or remove the foreign ion in organic hydrochloric acid;
Second step: by weight percent be the nano titanium oxide of 4.5% and the distilled water of 1/3rd to entering in reactor, fully stir under normal temperature, normal pressure, churning time is 12 minutes, and stirring velocity is 70 revs/min, and whipping temp is 14 DEG C;
3rd step: then add the iron trichloride that weight percent is 1.2%, fully stirs 7 minutes; Add the nitric acid that weight percent is 1.6%, fully stir 7 minutes; Add the distilled water of 1/3rd, fully stir 6 minutes; Add organic hydrochloric acid that weight percent is 3.3%, fully stir 7 minutes; Add the nonionogenic tenside that weight percent is 2.3%, fully stir 6 minutes; Add the stablizer that weight percent is 1.5%; Add the defoamer that weight percent is 5.6%, fully stir 7 minutes; Finally add residue distilled water again, then stir 10 minutes, stirring velocity is 55 revs/min, and whipping temp is 18 DEG C;
4th step: finally by the metre filter of obtained mixture through 0.12 μm, to remove the unwanted particles that particle diameter in mixture is greater than 0.12 μm, obtained required etching solution, its surface tension is low is 20 × 10
-3n/m.
Wherein, the concentration of described nitric acid is greater than 97.5% (weight percent), and the concentration of described organic hydrochloric acid is greater than 89% (weight percent).
Wherein, described nonionogenic tenside is spans nonionogenic tenside.
Wherein, described weakly acidic cation-exchange resin is slightly acidic styrene type cation exchange resin.
Wherein, the mass ratio of described weakly acidic cation-exchange resin and organic hydrochloric acid is 0.2 ~ 0.5.
In sum, the following advantage that liquid-crystal display etching solution of the present invention and preparation method thereof has: 1) change surface tension, make its surface tension be reduced to 20 ~ 40 from traditional 60mN/m
3about N/m, strengthens its surface wettability, and make the object in use reaching uniformity, etch effect is good, remains without microcrystal.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1., based on a preparation method for the circuit card etching solution of nano titanium oxide, it is characterized in that, comprise the steps:
The first step: weakly acidic cation-exchange resin being joined weight percent is in 2.5% ~ 3.3% organic hydrochloric acid, be uniformly mixed, the speed stirred is 50 ~ 60 revs/min, churning time is 5 ~ 7 minutes, whipping temp is 10 ~ 13 DEG C, then leach weakly acidic cation-exchange resin, control or remove the foreign ion in organic hydrochloric acid;
Second step: be that the nano titanium oxide of 2.5 ~ 4.5% and the distilled water of 1/3rd are to entering in reactor by weight percent, fully stir under normal temperature, normal pressure, churning time is 10 ~ 12 minutes, and stirring velocity is 60 ~ 70 revs/min, and whipping temp is 12 ~ 14 DEG C;
3rd step: then add the iron trichloride that weight percent is 0.5% ~ 1.2%, fully stir 6 ~ 7 minutes; Add the nitric acid that weight percent is 0.5 ~ 1.6%, fully stir 5 ~ 7 minutes; Add the distilled water of 1/3rd, fully stir 4 ~ 6 minutes; Add organic hydrochloric acid that weight percent is 2.5 ~ 3.3%, fully stir 5 ~ 7 minutes; Add the nonionogenic tenside that weight percent is 1.5 ~ 2.3%, fully stir 4 ~ 6 minutes; Add the stablizer that weight percent is 0.5 ~ 1.5%; Add the defoamer that weight percent is 3.5 ~ 5.6%, fully stir 3 ~ 7 minutes; Finally add residue distilled water again, then stir 8 ~ 10 minutes, stirring velocity is 45 ~ 55 revs/min, and whipping temp is 14 ~ 18 DEG C;
4th step: finally by the metre filter of obtained mixture through 0.12 μm, to remove the unwanted particles that particle diameter in mixture is greater than 0.12 μm, obtained required etching solution, its surface tension is low is 20 ~ 40 × 10-3N/m.
2. the preparation method of a kind of circuit card etching solution based on nano titanium oxide as claimed in claim 1, it is characterized in that, the concentration of described nitric acid is greater than 97.5% (weight percent), and the concentration of described organic hydrochloric acid is greater than 89% (weight percent).
3. the preparation method of a kind of circuit card etching solution based on nano titanium oxide as claimed in claim 1, it is characterized in that, described nonionogenic tenside is spans nonionogenic tenside.
4. the preparation method of a kind of circuit card etching solution based on nano titanium oxide as claimed in claim 1, it is characterized in that, described weakly acidic cation-exchange resin is slightly acidic vinylbenzene Zeo-karb.
5. the preparation method of a kind of circuit card etching solution based on nano titanium oxide as claimed in claim 1, it is characterized in that, the mass ratio of described weakly acidic cation-exchange resin and organic hydrochloric acid is 0.3 ~ 0.5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510946534.8A CN105525292A (en) | 2015-12-16 | 2015-12-16 | Nanometer-titania-based preparing method for etching liquid for circuit board |
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| CN201510946534.8A CN105525292A (en) | 2015-12-16 | 2015-12-16 | Nanometer-titania-based preparing method for etching liquid for circuit board |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107835577A (en) * | 2017-11-24 | 2018-03-23 | 无锡南理工新能源电动车科技发展有限公司 | A kind of preparation method of the display control circuit plate etching solution based on inorganic salts chloride |
| CN107937916A (en) * | 2017-11-24 | 2018-04-20 | 无锡南理工新能源电动车科技发展有限公司 | A kind of preparation method of the etching solution used for printed circuit board based on nanometer barium hydroxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108512A (en) * | 2009-12-25 | 2011-06-29 | 比亚迪股份有限公司 | Chemical etching liquid for metals and etching method |
| CN102181867A (en) * | 2011-04-11 | 2011-09-14 | 江阴市润玛电子材料有限公司 | Novel acidic molybdenum aluminum etching liquid and preparation process thereof |
| CN102766870A (en) * | 2011-05-06 | 2012-11-07 | 比亚迪股份有限公司 | Etching liquid and method for etching flexible circuit board |
| CN103160207A (en) * | 2011-12-16 | 2013-06-19 | 安集微电子（上海）有限公司 | Metal chemico-mechanical polishing sizing agent and application thereof |
-
2015
- 2015-12-16 CN CN201510946534.8A patent/CN105525292A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108512A (en) * | 2009-12-25 | 2011-06-29 | 比亚迪股份有限公司 | Chemical etching liquid for metals and etching method |
| CN102181867A (en) * | 2011-04-11 | 2011-09-14 | 江阴市润玛电子材料有限公司 | Novel acidic molybdenum aluminum etching liquid and preparation process thereof |
| CN102766870A (en) * | 2011-05-06 | 2012-11-07 | 比亚迪股份有限公司 | Etching liquid and method for etching flexible circuit board |
| CN103160207A (en) * | 2011-12-16 | 2013-06-19 | 安集微电子（上海）有限公司 | Metal chemico-mechanical polishing sizing agent and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107835577A (en) * | 2017-11-24 | 2018-03-23 | 无锡南理工新能源电动车科技发展有限公司 | A kind of preparation method of the display control circuit plate etching solution based on inorganic salts chloride |
| CN107937916A (en) * | 2017-11-24 | 2018-04-20 | 无锡南理工新能源电动车科技发展有限公司 | A kind of preparation method of the etching solution used for printed circuit board based on nanometer barium hydroxide |
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Application publication date: 20160427 |
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